CN104830524A - Method for extracting alpha-linolenic acid from perilla seed in one step - Google Patents
Method for extracting alpha-linolenic acid from perilla seed in one step Download PDFInfo
- Publication number
- CN104830524A CN104830524A CN201510211616.8A CN201510211616A CN104830524A CN 104830524 A CN104830524 A CN 104830524A CN 201510211616 A CN201510211616 A CN 201510211616A CN 104830524 A CN104830524 A CN 104830524A
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- CN
- China
- Prior art keywords
- alpha
- linolenic acid
- liquid phase
- perilla seed
- ethanol
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
- C11B1/04—Pretreatment of vegetable raw material
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/12—Refining fats or fatty oils by distillation
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C1/00—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids
- C11C1/02—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids from fats or fatty oils
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C1/00—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids
- C11C1/08—Refining
- C11C1/10—Refining by distillation
- C11C1/103—Refining by distillation after or with the addition of chemicals
Abstract
The invention discloses a method for extracting alpha-linolenic acid from perilla seed in one step. The method comprises the following steps: taking perilla seeds as the raw material, grinding perilla seeds, sieving; using an ethanol-alkali solution to extract grinded perilla seeds in an extraction pot; cooling to a temperature of 10 to 50 DEG C, filtering, collecting the liquid phase, adjusting the pH value of the liquid phase by hydrochloric acid; finally washing the liquid phase by a saturated saline solution until the liquid phase becomes neutral, condensing the liquid phase to remove alcohol and water, and carrying out molecular distillation to obtain the alpha-linolenic acid product; wherein the acid value of the obtain product is 187 KOHmg/g, and the alpha-linolenic acid content is not less than 65%. The provided method has the following advantages: the technology is simplified, and the steps for extracting alpha-linolenic acid from perilla seeds are reduced; the fatty acid yield (around 50%) is high, and no fatty acid is left in residues; the quality of the obtained alpha-linolenic acid is high, the linolenic acid is not destroyed, the acid value is about 187 KOHmg/g, and the alpha-linolenic content is not less than 65%.
Description
Technical field
The present invention relates to the method that perilla seed single stage method extracts alpha-linolenic acid, the specifically direct method extracting alpha-linolenic acid from perilla seed.
Background technology
Alpha-linolenic acid is all-cis formula 9,12, and 15 punicic acids, are very easily oxidized, and accelerates with the rising oxidation rate of temperature when not having protection.At present, in suitability for industrialized production high-content alpha-linolenic acid product, be mainly raw material with perilla seed, in perilla seed, alpha-linolenic acid content accounts for 65% of total fat, obtain Purple Perilla Seed Oil through squeezing/leaching, more just can obtain alpha-linolenic acid product through saponification, acidifying, washing, dehydration, molecular distillation.Perilla seed oil-containing about 50%, in the process producing oil, adopts squeezing/leaching to obtain vegetables oil, the Purple Perilla Seed Oil oil yield that milling process is produced is low, is only about 45%, containing higher in the dregs of rice, alpha-linolenic acid is caused to waste, and need high temperature, cause alpha-linolenic acid to destroy, energy waste is large, cost is higher, in addition alpha-linolenic acid No. six dissolvent residuals of producing with No. six solvents of extraction process are higher, and cause high temperature precipitation difficulty, alpha-linolenic acid destroys serious.
Summary of the invention
The object of the invention is to be to overcome the deficiencies in the prior art, and provide a kind of perilla seed single stage method to extract the method for alpha-linolenic acid, eliminate traditional squeezing/leaching and first produce Purple Perilla Seed Oil step, save the expense and alpha-linolenic acid loss that produce in liquefaction process, reduce cost.For reaching above-mentioned purpose, present invention employs following technical scheme:
Perilla seed single stage method extracts the method for alpha-linolenic acid, it is characterized in that: take perilla seed as raw material, through pulverizing and sieving; In extractor, the perilla seed after pulverizing is extracted with ethanol-alkaline solution; Be cooled to 10-50 DEG C and cross leaching liquid phase, then regulate the pH value of liquid phase with hydrochloric acid; Finally extremely neutral by saturated aqueous common salt washing liquid phase, concentrated dealcoholysis, water, obtaining acid number by molecular distillation is 187KOHmg/g, the alpha-linolenic acid product of alpha-linolenic acid content >=65%.
Described perilla seed requires moldy kernel≤0.3%, and impurity≤2.0%, moisture≤9.0%, pulverized 60-90 mesh sieve.
Described ethanol-alkaline solution, ethanol, alkali are necessary for food grade, and alcohol concn is 40%-80%, and in ethanol-alkaline solution, alkali content is 5%-20%.
Described ethanol-alkaline solution extracts the perilla seed after pulverizing in extractor, and the ratio (volume ratio or mass ratio) of the perilla seed after pulverizing and ethanol-alkaline solution is 1: 0.5-2, and extraction temperature is 70 DEG C-85 DEG C, extraction time 2-8 hour.
Described hydrochloric acid regulates the pH value of liquid phase, and hydrochloric acid is food grade, regulates liquid phase pH value to 2-4.
Described saturated common salt water temp is 50-80 DEG C, and liquid phase and saturated aqueous common salt ratio (the same) are 1: 0.5-2.2.
After adopting such scheme, the present invention has the following advantages:
Save the step producing Purple Perilla Seed Oil, Simplified flowsheet; Lipid acid yield is high, is about 50%, is zero lipid acid in residue; Obtain alpha-linolenic acid product quality high, alpha-linolenic acid is not damaged, and acid number KOHmg/g is about 187, alpha-linolenic acid content >=65%.
Embodiment
The present invention relates to the method that perilla seed single stage method extracts alpha-linolenic acid, comprise the following steps:
Be raw material with perilla seed, pulverize and sieve; In extractor, the perilla seed after pulverizing is extracted with ethanol-alkaline solution; Be cooled to 10-50 DEG C and cross leaching liquid phase, then regulate the pH value of liquid phase with hydrochloric acid; Finally extremely neutral by saturated aqueous common salt washing liquid phase, concentrated dealcoholysis, water, obtaining acid number by molecular distillation is 187KOHmg/g, the alpha-linolenic acid product of alpha-linolenic acid content >=65%.
Wherein perilla seed requires moldy kernel≤0.3%, and impurity≤2.0%, moisture≤9.0%, pulverized 60-90 mesh sieve.
Ethanol-alkaline solution, ethanol, alkali are necessary for food grade, and alcohol concn is 40%-80%, and in ethanol-alkaline solution, alkali content is 5%-20%.
Ethanol-alkaline solution extracts the perilla seed after pulverizing in extractor, and the ratio of the perilla seed after pulverizing and ethanol-alkaline solution is 1: 0.5-2, and extraction temperature is 70 DEG C-85 DEG C, extraction time 2-8 hour.
Regulate the pH value of liquid phase with hydrochloric acid, hydrochloric acid is food grade, regulates liquid phase pH value to 2-4.
Saturated common salt water temp is 50-80 DEG C, and liquid phase and saturated aqueous common salt ratio are 1: 0.5-2.2.
The present invention utilizes the alpha-linolenic acid in ethanol-alkaline solution saponification-extraction single stage method extraction perilla seed, reach according to the saponification value of fat in perilla seed and the ratio of oleaginousness determination alkali and ethanol the object extracted completely, then obtain the method for alpha-linolenic acid product by acidifying, washing, dehydration, molecular distillation.
Below enumerate specific embodiment to illustrate method steps of the present invention.Wherein, raw material is perilla seed, requires moldy kernel≤0.3%, impurity≤2.0%, moisture≤9.0%.The ethanol selected is edible ethanol, and alkali, hydrochloric acid, salt are food grade.For the detection of alpha-linolenic acid acid number, adopt the mensuration of GB/T 5530 animal-plant oil acid number and acidity, the mensuration of alpha-linolenic acid content adopts the gas chromatographic analysis of the preparation of GB/T 17376 animal-plant oil fatty acid methyl ester and GB/T 17377 animal-plant oil Fatty acid methyl ester.
Embodiment 1:
Be in the ethanolic soln of 40% by 25KG alkali dissolution and 475L concentration, mix, squeeze in extractor; 1000KG perilla seed is pulverized 60 mesh sieves, puts into extractor; Be warming up to 70 DEG C, keep extraction 2 hours; Be cooled to 10 DEG C and cross leaching liquid phase, then regulate the pH value of liquid phase to be 2 with hydrochloric acid; Finally extremely neutral by 1100KG saturated aqueous common salt washing liquid phase, vacuum concentration dealcoholysis, water, pass through molecular distillation.Obtaining acid number is 187KOHmg/g, and alpha-linolenic acid content is the alpha-linolenic acid product 500KG of 65%.
Embodiment 2:
Be in the ethanolic soln of 80% by 100KG alkali dissolution and 1900L concentration, mix, squeeze in extractor; 1000KG perilla seed is pulverized 80 mesh sieves, puts into extractor; Be warming up to 85 DEG C, keep extraction 8 hours; Be cooled to 50 DEG C and cross leaching liquid phase, then regulate the pH value of liquid phase to be 4 with hydrochloric acid; Finally extremely neutral by 1000KG saturated aqueous common salt washing liquid phase, vacuum concentration dealcoholysis, water, pass through molecular distillation.Obtaining acid number is 187KOHmg/g, and alpha-linolenic acid content is the alpha-linolenic acid product 510KG of 67%.
Embodiment 3:
Be in the ethanolic soln of 80% by 25KG alkali dissolution and 475L concentration, mix, squeeze in extractor; 1000KG perilla seed is pulverized 80 mesh sieves, puts into extractor; Be warming up to 70 DEG C, keep extraction 8 hours; Be cooled to 50 DEG C and cross leaching liquid phase, then regulate the pH value of liquid phase to be 4 with hydrochloric acid; Finally extremely neutral by 1100KG saturated aqueous common salt washing liquid phase, vacuum concentration dealcoholysis, water, pass through molecular distillation.Obtaining acid number is 187KOHmg/g, and alpha-linolenic acid content is the alpha-linolenic acid product 490KG of 65.5%.
Embodiment 4:
Be in the ethanolic soln of 60% by 50KG alkali dissolution and 1000L concentration, mix, squeeze in extractor; 1000KG perilla seed is pulverized 70 mesh sieves, puts into extractor; Be warming up to 80 DEG C, keep extraction 4 hours; Be cooled to 50 DEG C and cross leaching liquid phase, then regulate the pH value of liquid phase to be 3 with hydrochloric acid; Finally extremely neutral by 1000KG saturated aqueous common salt washing liquid phase, vacuum concentration dealcoholysis, water, pass through molecular distillation.Obtaining acid number is 187KOHmg/g, and alpha-linolenic acid content is the alpha-linolenic acid product 505KG of 66%.
Claims (2)
1. perilla seed single stage method extracts the method for alpha-linolenic acid, it is characterized in that: comprise the following steps: be raw material with perilla seed, pulverizes and sieves; In extractor, the perilla seed after pulverizing is extracted with ethanol-alkaline solution; Be cooled to 10-50 DEG C and cross leaching liquid phase, then regulate the pH value of liquid phase with hydrochloric acid; Finally extremely neutral by saturated aqueous common salt washing liquid phase, concentrated dealcoholysis, water, obtaining acid number by molecular distillation is 187KOHmg/g, the alpha-linolenic acid product of alpha-linolenic acid content >=65%;
Wherein perilla seed requires moldy kernel≤0.3%, impurity≤2.0%, and moisture≤9.0%, pulverized 60-90 mesh sieve;
Ethanol-alkaline solution, ethanol, alkali are necessary for food grade, and alcohol concn is 40%-80%, and in ethanol-alkaline solution, alkali content is 5%-20%;
Ethanol-alkaline solution extracts the perilla seed after pulverizing in extractor, and the ratio of the perilla seed after pulverizing and ethanol-alkaline solution is 1: 0.5-2, and extraction temperature is 70 DEG C-85 DEG C, extraction time 2-8 hour;
Regulate the pH value of liquid phase with hydrochloric acid, hydrochloric acid is food grade, regulates liquid phase pH value to 2-4;
Saturated common salt water temp is 50-80 DEG C, and liquid phase and saturated aqueous common salt ratio are 1: 0.5-2.2.
2. perilla seed single stage method extracts the method for alpha-linolenic acid, it is characterized in that: extract the alpha-linolenic acid in perilla seed by ethanol-alkaline solution saponification-extraction single stage method, reach according to the saponification value of fat in perilla seed and the ratio of oleaginousness determination alkali and ethanol the object extracted completely, then obtain the method for alpha-linolenic acid product by acidifying, washing, dehydration, molecular distillation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510211616.8A CN104830524A (en) | 2015-04-23 | 2015-04-23 | Method for extracting alpha-linolenic acid from perilla seed in one step |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510211616.8A CN104830524A (en) | 2015-04-23 | 2015-04-23 | Method for extracting alpha-linolenic acid from perilla seed in one step |
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| Publication Number | Publication Date |
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| CN104830524A true CN104830524A (en) | 2015-08-12 |
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| CN201510211616.8A Pending CN104830524A (en) | 2015-04-23 | 2015-04-23 | Method for extracting alpha-linolenic acid from perilla seed in one step |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2017186502A (en) * | 2016-04-01 | 2017-10-12 | ブリリアント バイオメディカル カンパニー リミテッド | Camellia oil and manufacturing method therefor |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63216845A (en) * | 1987-03-05 | 1988-09-09 | Agency Of Ind Science & Technol | Concentration of gamma-linolenic acid |
| CN1837179A (en) * | 2005-12-30 | 2006-09-27 | 安阳化学工业集团有限责任公司 | Process for preparing alpha-linolenic acid with purity more than 80% |
| CN102978009A (en) * | 2012-11-26 | 2013-03-20 | 安徽亿源生物工程有限公司 | Preparation method of linseed oil |
-
2015
- 2015-04-23 CN CN201510211616.8A patent/CN104830524A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63216845A (en) * | 1987-03-05 | 1988-09-09 | Agency Of Ind Science & Technol | Concentration of gamma-linolenic acid |
| CN1837179A (en) * | 2005-12-30 | 2006-09-27 | 安阳化学工业集团有限责任公司 | Process for preparing alpha-linolenic acid with purity more than 80% |
| CN102978009A (en) * | 2012-11-26 | 2013-03-20 | 安徽亿源生物工程有限公司 | Preparation method of linseed oil |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2017186502A (en) * | 2016-04-01 | 2017-10-12 | ブリリアント バイオメディカル カンパニー リミテッド | Camellia oil and manufacturing method therefor |
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Application publication date: 20150812 |
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